FREEZE DRYING

INTRODUCTION
Drying is used to remove moisture, typically water from a material
or component, usually in conjunction with a heating process
Freeze drying involves the removal of water or other solvent from a
frozen product by a process called sublimation
freeze drying, the material does not go through the liquid phase,
and it allows the preparation of a stable product that is easy to use
and aesthetic in appearance

Freeze Dryer
material is held on shelves or belts in a chamber that is under
high vacuum
food is frozen before being loaded into the dryer
Heat transfer is by conduction or radiation
the vapour is removed by vacuum pump and condensed
In accelerated freeze drying
Heat transfer by conduction
Pieces of food are shaped



Principles
Consist of 3 stages
Prefreezing
Primary drying (sublimation)
Secondary drying

Prefreezing
Materials must first be completely prefrozen
Product freeze in two ways, depending on the composition of
the product
changes occur in the solute concentrations of product
is not completely frozen until all solute in the suspension is
frozen
Primary Drying
the shift from a solid directly into a gas
the machine runs the compressors to lower the temperature
the machine turns on the vacuum pump to force air out of the
chamber
The water vapor condenses onto the freezing coil in solid ice
form

The process takes so long because overheating the material
can significantly change the composition and structure
100% removal of water is needed during the packaging in
order to maintain the quality.

Secondary Drying
bound moisture is still present in the product
Drying is continued at warmer temperature
isothermal desroption
the vacuum should be at the lowest and the condenser
temperature must be at the coolest
Half the time pf primary drying
Equations
Heat flux to the surface(steady state):
q = h(T
e
-T
s
) =

(T
s
-T
f
) (A)
mass flux of the water vapor from the sublimation
N
A
=

)=

) (B)
Rearrange A,
q =
1
1

(T
e
T
f
) (C)



The heat flux and mass flux at steady-state are related by
q = H
s
N
A
(D)
L = (1 x)

2
(E)
The rate of freeze-drying can be related to N
A
by
N
A
=

2
1

) (F)
Combining equation B, C, D and E, heat transfer obtain is

2
1

) =
1
1

+ 1

(T
e
T
f
) (G)
Integrating F
t =

2
4

(
1

1
2
2

2
2
2
) (H)



Requirements
There are four requirement for freeze-drying :
Object is frozen solid
Condensing surface is colder than the object to be
freeze-dry
Vacuum pump that produce very low absolute
pressure
Heat source
What Happens Inside?
A frozen object is placed inside a chamber
chamber provides condensing surface
pump is turned on and the inside of the chamber reaches
proper pressure
vapor of moisture is extracted from the object and collected
on the condenser
After certain time, heat is slowly exposed to the product,
which helps extracting more vapours and eliminate bound
water.

Objects Ideal to be freeze dry
for recovery of water-damaged books, documents, artwork,
keepsakes
preservation of animals, floral products, food and drugs


Ideal characteristic of freeze dryer
the chamber is made out of borosilicate glass
the condenser can act as trap to collect the water vapour
released from the product in the drying chamber
the condenser is also used to protect the vacuum pump from
water vapour
Condenser also helps establish a vapour trail from the product
out of the drying chamber
Advantages
with freeze-drying the consistency, shape, colour and the
intense flavour of the original product remain unaltered
the products become much lighter
the original structure of the products remains unaltered
Difference
Freeze Dryer Spray Dryer
Dryers for particulates and granular
solids

Dryers for slurries and suspensions

To minimize drying times, freeze dryers
are program-controlled
may use low pressure chambers to
enhance drying rates
Vacuum pressure is typically under 25
Pa and the condenser operates at
around 40C

Most spray dryers operate at slight
negative pressure
APPLICATIONS
Pharmaceutical and biotechnology
Pharmaceutical companies often use freeze-drying to increase
the shelf life of the products, such as vaccines and other
injectable
Food Industry
Freeze-drying is used to preserve food, the resulting product
being very lightweight
Technological industry
In chemical synthesis, products are often freeze-dried to make
them more stable, or easier to dissolve in water for subsequent
use
In bio separations, freeze-drying can be used also as a late-stage
purification procedure, because it can effectively remove solvents